CN109592703B - CuO/Cu2O-La2O3Preparation method of multiphase composite sol - Google Patents
CuO/Cu2O-La2O3Preparation method of multiphase composite sol Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 18
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims description 28
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 12
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 12
- QPLDLSVMHZLSFG-UHFFFAOYSA-N CuO Inorganic materials [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001263 FEMA 3042 Substances 0.000 claims description 4
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 235000015523 tannic acid Nutrition 0.000 claims description 4
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical group OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 4
- 229940033123 tannic acid Drugs 0.000 claims description 4
- 229920002258 tannic acid Polymers 0.000 claims description 4
- 235000004515 gallic acid Nutrition 0.000 claims description 3
- 229940074391 gallic acid Drugs 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 239000011248 coating agent Substances 0.000 abstract description 16
- 238000000576 coating method Methods 0.000 abstract description 16
- 238000009690 centrifugal atomisation Methods 0.000 abstract description 15
- 238000011084 recovery Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 7
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 2
- 239000002120 nanofilm Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 41
- 238000005507 spraying Methods 0.000 description 16
- 230000035945 sensitivity Effects 0.000 description 15
- 229910044991 metal oxide Inorganic materials 0.000 description 8
- 150000004706 metal oxides Chemical class 0.000 description 8
- 238000001514 detection method Methods 0.000 description 6
- 238000000889 atomisation Methods 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000002103 nanocoating Substances 0.000 description 5
- 230000004044 response Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0037—NOx
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
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- Medicinal Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to the field of gas-sensitive materials, and aims to provide CuO/Cu2O‑La2O3A preparation method of multiphase composite sol. The method comprises the following steps: mixing nano CuO sol and nano Cu2Reacting the O sol at 60-120 ℃, and adding restricted space molecules; after fully and uniformly mixing, adding the nano La dropwise2O3Sol; then carrying out sol reaction for 8-14 h at the temperature of 25-50 ℃ to finally obtain CuO/Cu2O‑La2O3And (3) multiphase composite sol. The invention adopts nano sol particles and rare earth oxide as modification components, utilizes nano activity effect and unique physicochemical properties of rare earth, prepares the high-dispersion type multiphase composite nano sol in a confined space molecular structure, and solves the problem of easy agglomeration of the traditional nano sol. If a centrifugal atomization method coating technology is further adopted, the controllable preparation of the high-quality and uniform multi-phase composite nano-film layer can be realized, and the NO of the material can be effectively improvedxSensitivity of gas, response-recovery characteristics.
Description
Technical Field
The invention relates to the field of gas-sensitive materials, in particular to CuO/Cu2O-La2O3A preparation method of multiphase composite sol.
Background
The atmospheric pollution seriously threatens the health and survival of human beings, and the metal oxide gas sensor becomes an effective means for detecting harmful gases in the atmosphere due to the advantages of simple equipment, small volume, quick response, high sensitivity, low cost and the like. And as the core of the gas sensor, the gas sensitive material determines the detection and the use performance of the gas sensor. Conventional metal oxide gas sensing materials have earlier-discovered SnO2ZnO, alpha-iron oxide, gamma-iron oxide, and the like. However, the conventional gas sensitive material with a single component has certain limitations in detecting the type and sensitivity of gas, such as low sensitivity, low selectivity and the like, so some researchers improve the characteristics of the gas sensitive material, such as detection sensitivity and the like by doping trace elements, such as rare earth elements, adding different oxides and the like.
The nano material has certain advantages in the high-sensitivity application of the gas sensitive material due to the nano effects of high specific surface area, high chemical activity sites and the like. The smaller the particle size of the material particles, the larger the quantity and energy participating in the gas-sensitive reaction, and the more remarkable the gas-sensitive property is. Therefore, the gas sensitive element with excellent evaluation indexes such as sensitivity, selectivity, stability, response recovery characteristics and the like can be prepared by accurately controlling the chemical properties such as the component composition, the micro-morphology, the grain size, the crystallinity, the doping component and the like of the gas sensitive material.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a CuO/Cu2O-La2O3A preparation method of multiphase composite sol.
In order to solve the technical problem, the solution of the invention is as follows:
provides a CuO/Cu2O-La2O3The preparation method of the multiphase composite sol comprises the following steps:
(1) according to the formula CuO and Cu2Taking nano CuO sol and nano Cu according to the molar ratio of O being 1: 12Adding the O sol into a reaction kettle, and reacting for 4-18 h at the temperature of 60-120 ℃;
(2) introducing a reaction product into a round-bottom flask, and adding a restricted space molecule under the stirring condition; after fully and uniformly mixing, adding the nano La dropwise2O3Sol; then carrying out sol reaction for 8-14 h at the temperature of 25-50 ℃ to finally obtain CuO/Cu2O-La2O3Multi-phase composite sol;
the restricted space molecule accounts for CuO and Cu2O and La2O3The mol percentage of the total solid content of the sol is 1-3%, and the nano La2O3La in the sol2O3Account for CuO and Cu2O and La2O3The mol percentage of the total solid content of the sol is 9-22%.
In the present invention, the solid content of the nano CuO sol is 0.5%.
In the invention, the nano Cu2The solids content of the O sol was 2%.
In the invention, the nano La is2O3The solids content of the sol was 1.5%.
In the present invention, the constrained space molecule is tannic acid, gallic acid, or polyethylene glycol (PEG 2000).
In the present invention, the stirring is magnetic stirring.
Description of the inventive principles:
the invention prepares the CuO/Cu2O-La2O3 multiphase composite nano sol with high dispersibility in a limited space molecular structure by utilizing a nano-dispersion combined rare earth doping modification composite technology. The nano sol can be further used as a precursor, the uniform coating of the nano sol is realized by adopting a centrifugal atomization method, and the nano sol has excellent sensitivity and response-recovery characteristics on the atmosphere pollution gas NOx.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts nano sol particles and rare earth oxide as modification components, and utilizes the nano activity effect and the unique physicochemical property of rare earth to prepare the high-dispersion CuO/Cu in the molecular structure of the restricted space2O-La2O3The multiphase composite nano sol solves the problem of easy agglomeration of the traditional nano sol.
(2) CuO/Cu obtained by the invention2O-La2O3The multiphase composite sol can further adopt a centrifugal atomization coating technology to realize high-quality and uniform CuO/Cu2O-La2O3Controllable preparation of multiphase composite nano coating, effectively improving NO of materialxSensitivity of gas, response-recovery characteristics.
Detailed Description
The nano CuO sol and the nano Cu are prepared by the method2O sol, nano La2O3The sol is prepared by the prior art and can be prepared by the conventional preparation method.
CuO/Cu prepared by the invention2O-La2O3A heterogeneous composite sol, which may furtherThe method is used for preparing the gas sensitive material coating. The coating is obtained by spraying a metal oxide gas-sensitive element by using a centrifugal atomization method, and specific examples are as follows:
CuO/Cu prepared by using the method2O-La2O3And (3) spraying the multiphase composite sol on the metal oxide gas-sensitive element by a centrifugal atomization method to obtain a gas-sensitive material coating on the surface of the element. The operating parameters of the centrifugal atomization spraying can be selected as follows: the centrifugal rate is 3000-5000 r/min; the atomization air pressure is 0.2-0.65 MPa; the spraying distance is 100-300 mm.
Example 1
(1) According to the formula CuO and Cu2Taking nano CuO sol and nano Cu according to the molar ratio of O being 1: 12Adding the O sol into a reaction kettle, and reacting for 18 hours at the temperature of 60 ℃;
(2) introducing a reaction product into a round-bottom flask, and adding a restricted space molecule under the stirring condition; after fully and uniformly mixing, adding the nano La dropwise2O3Sol; then carrying out sol reaction for 14h at the temperature of 25 ℃ to finally obtain CuO/Cu2O-La2O3Multi-phase composite sol;
the nano Cu2The solid content of the O sol is 2 percent, and the nano La2O3The solid content of the sol was 1.5%, and the solid content of the nano CuO sol was 0.5%. The restricted space molecule is tannic acid, and accounts for CuO and Cu2O and La2O3The mol percentage of the total solid content of the sol is 1 percent; nano La2O3La in the sol2O3Account for CuO and Cu2O and La2O3The molar percentage of the total solid content of the sol was 9%.
Preparation and performance evaluation of the coating:
(1) using the CuO/Cu obtained in this example2O-La2O3And (3) spraying the multiphase composite sol on the metal oxide gas-sensitive element by a centrifugal atomization method to obtain a gas-sensitive material coating on the surface of the element. The operating parameters of the centrifugal atomization spraying are as follows: the centrifugal rate is 3000 r/min; the atomization air pressure is 0.2 MPa; the spraying distance is 100 mm.
(2) To pairPrepared CuO/Cu2O-La2O3Heterogeneous composite nanocoating for NOxThe gas sensitivity characteristics (including sensitivity, response-recovery characteristics, etc.) of the gas are evaluated for detection.
Example 2
(1) According to the formula CuO and Cu2Taking nano CuO sol and nano Cu according to the molar ratio of O being 1: 12Adding the O sol into a reaction kettle, and reacting for 4 hours at 120 ℃;
(2) introducing a reaction product into a round-bottom flask, and adding a restricted space molecule under the stirring condition; after fully and uniformly mixing, adding the nano La dropwise2O3Sol; then carrying out sol reaction for 8h at the temperature of 50 ℃ to finally obtain CuO/Cu2O-La2O3Multi-phase composite sol;
the solid content of the nano CuO sol is 0.5 percent, and the nano Cu2The solid content of the O sol is 2 percent, and the nano La2O3The solids content of the sol was 1.5%. The confined space molecule is gallic acid, and accounts for CuO and Cu2O and La2O3The mol percentage of the total solid content of the sol is 3 percent; nano La2O3La in the sol2O3Account for CuO and Cu2O and La2O3The molar percentage of the total solid content of the sol was 22%.
Preparation and performance evaluation of the coating:
(1) using the CuO/Cu obtained in this example2O-La2O3And (3) spraying the multiphase composite sol on the metal oxide gas-sensitive element by a centrifugal atomization method to obtain a gas-sensitive material coating on the surface of the element. The operating parameters of the centrifugal atomization spraying are as follows: the centrifugal rate is 5000 r/min; the atomization air pressure is 0.65 MPa; the spraying distance is 300 mm.
(2) For the prepared CuO/Cu2O-La2O3Heterogeneous composite nanocoating for NOxThe gas sensitivity characteristics (including sensitivity, response-recovery characteristics, etc.) of the gas are evaluated for detection.
Example 3
(1) According to the formula CuO and Cu2Taking nano CuO sol and nano CuO sol with the molar ratio of O being 1: 1Cu2Adding the O sol into a reaction kettle, and reacting for 12 hours at 90 ℃;
(2) introducing a reaction product into a round-bottom flask, and adding a restricted space molecule under the stirring condition; after fully and uniformly mixing, adding the nano La dropwise2O3Sol; then carrying out sol reaction for 10h at the temperature of 40 ℃ to finally obtain CuO/Cu2O-La2O3Multi-phase composite sol;
the solid content of the nano CuO sol is 0.5 percent, and the nano Cu2The solid content of the O sol is 2 percent, and the nano La2O3The solids content of the sol was 1.5%. The restricted space molecule is polyethylene glycol (PEG2000) occupying CuO and Cu2O and La2O3The mol percentage of the total solid content of the sol is 2 percent, and the nano La2O3La in the sol2O3Account for CuO and Cu2O and La2O3The molar percentage of the total solid content of the sol was 12%.
Preparation and performance evaluation of the coating:
(1) using the CuO/Cu obtained in this example2O-La2O3And (3) spraying the multiphase composite sol on the metal oxide gas-sensitive element by a centrifugal atomization method to obtain a gas-sensitive material coating on the surface of the element. The operating parameters of the centrifugal atomization spraying are as follows: the centrifugal rate is 4000 r/min; the atomization air pressure is 0.45 MPa; the spraying distance is 200 mm.
(2) For the prepared CuO/Cu2O-La2O3Heterogeneous composite nanocoating for NOxThe gas sensitivity characteristics (including sensitivity, response-recovery characteristics, etc.) of the gas are evaluated for detection.
Comparative example 4
(1) According to the formula CuO and Cu2Taking nano CuO sol and nano Cu according to the molar ratio of O being 1: 12Adding the O sol into a reaction kettle, and reacting for 12 hours at 90 ℃;
(2) introducing a reaction product into a round-bottom flask, and adding a restricted space molecule under the stirring condition; after fully and uniformly mixing, carrying out sol reaction for 10h at the temperature of 40 ℃ to finally obtain CuO/Cu2O composite sol;
the solid content of the nano CuO sol is 0.5 percent, and the nano Cu2The solids content of the O sol was 2%. The restricted space molecule is tannic acid, and accounts for CuO and Cu2The mol percentage of the total solid content of the O sol is 1.5 percent, and the nano La2O3La in the sol2O3Is 0%.
Preparation and performance evaluation of the coating:
(1) using the CuO/Cu obtained in this example2And spraying the O composite sol on the metal oxide gas-sensitive element by a centrifugal atomization method to obtain a coating on the surface of the element. The operating parameters of the centrifugal atomization spraying are as follows: the centrifugal rate is 3500 r/min; the atomization air pressure is 0.25 MPa; the spraying distance is 150 mm.
(2) For the prepared CuO/Cu2O composite nanolayered coating with NOxThe gas sensitivity characteristics (including sensitivity, response-recovery characteristics, etc.) of the gas are evaluated for detection.
The invention utilizes the nanometer active effect and the unique physicochemical property of rare earth to successfully prepare the high-dispersion CuO/Cu in the molecular structure of the restricted space2O-La2O3The multiphase composite nano sol solves the problem of easy agglomeration of the traditional nano sol. Simultaneously, the centrifugal atomization coating technology can realize high-quality and uniform CuO/Cu2O-La2O3Controllable preparation of multiphase composite nano coating, effectively improving NO of materialxSensitivity of gas, response-recovery characteristics. Also, the results from the examples show that: gas sensitive materials prepared in examples 1 and 2 used in the present invention for NOxThe sensitivity and response-recovery characteristics of the gas are more excellent.
The results of the gas sensitive property test of each example are shown in the following table:
table 1 gas sensitive property test results of each example
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention.
Claims (5)
1. CuO/Cu2O-La2O3The preparation method of the multiphase composite sol is characterized by comprising the following steps:
(1) according to the formula CuO and Cu2Taking nano CuO sol and nano Cu according to the molar ratio of O being 1: 12Adding the O sol into a reaction kettle, and reacting for 4-18 h at the temperature of 60-120 ℃;
(2) introducing a reaction product into a round-bottom flask, and adding a restricted space molecule under the stirring condition; after fully and uniformly mixing, adding the nano La dropwise2O3Sol; then carrying out sol reaction for 8-14 h at the temperature of 25-50 ℃ to finally obtain CuO/Cu2O-La2O3Multi-phase composite sol;
the restricted space molecule is tannic acid, gallic acid or polyethylene glycol, and the restricted space molecule accounts for CuO and Cu2O and La2O3The mol percentage of the total solid content of the sol is 1-3%; nano La2O3La in the sol2O3Account for CuO and Cu2O and La2O3The mol percentage of the total solid content of the sol is 9-22%.
2. The method according to claim 1, wherein the nano CuO sol has a solid content of 0.5%.
3. The method of claim 1, wherein the nanocu2The solids content of the O sol was 2%.
4. The method of claim 1, wherein the nano-La is2O3The solids content of the sol was 1.5%.
5. The method of claim 1, wherein the stirring is magnetic stirring.
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